CN107245317B - Moisture-curing polyurethane hot melt adhesive and preparation method thereof - Google Patents
Moisture-curing polyurethane hot melt adhesive and preparation method thereof Download PDFInfo
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- C09J175/00—Adhesives based on polyureas or polyurethanes; Adhesives based on derivatives of such polymers
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- C08G18/6666—Compounds of group C08G18/48 or C08G18/52
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Abstract
The invention relates to a moisture-curing polyurethane hot melt adhesive and a preparation method thereof. The moisture-curing polyurethane hot melt adhesive comprises the following raw materials in parts by weight: 20-30 parts of polyethylene glycol 200, 10-20 parts of 1, 4-butanediol, 10-30 parts of polyisocyanate, 5-10 parts of ethyl trichlorosilane, 0.5-3 parts of cerium trichloride, 5-12 parts of plasticizer, 2-6 parts of stabilizer, 0.1-2 parts of antioxidant, 0-18 parts of colorant, 10-20 parts of catalyst and 0-20 parts of filler, wherein the polyisocyanate is selected from MDI and/or HDI, and the catalyst is selected from nano titanium dioxide and/or nano calcium carbonate. The moisture-curable polyurethane hot melt adhesive has the characteristics of strong initial adhesion, high bonding strength, good toughness, strong permeability and affinity, can resist high temperature, and can be suitable for firmly bonding substrates such as metal, plastic, glass and the like. The preparation method of the moisture curing type polyurethane hot melt adhesive is simple and reliable, and the gluing is convenient.
Description
Technical Field
The invention relates to the field of electronic adhesives, in particular to a moisture-curing type polyurethane hot melt adhesive and a preparation method thereof.
Background
The hot melt adhesive is a plastic adhesive, the physical state of which changes along with the change of temperature within a certain temperature range, and the chemical property of which is unchanged, is nontoxic and tasteless, and belongs to an environment-friendly chemical product. Among them, moisture-curable polyurethane hot melt adhesives are widely used. However, the adhesive strength and toughness of the existing moisture-curable polyurethane hot melt adhesive still need to be improved.
Disclosure of Invention
Accordingly, there is a need for a moisture-curable hot melt adhesive having high adhesive strength and good flexibility, and a method for preparing the same.
The moisture-curing polyurethane hot melt adhesive comprises the following raw materials in parts by weight:
wherein the polyisocyanate is selected from 4,4' -diphenylmethane diisocyanate (MDI) and/or hexane-1, 6-diisocyanate (HDI), and the catalyst is selected from nano titanium dioxide and/or nano calcium carbonate.
In one embodiment, the polyisocyanate is MDI and HDI in a weight ratio of 7-9: 19-21.
In one embodiment, the plasticizer is selected from at least one of di-n-octyl phthalate, butyl benzyl phthalate, di-sec-octyl phthalate, and dicyclohexyl phthalate.
In one embodiment, the antioxidant is selected from at least one of 4-hydroxyoctadecanoic acid anilide, 4 '-thiobis (3-methyl-6-tert-butylphenol), and 2, 2' -methylenebis (4-methyl-6-tert-butylphenol).
In one embodiment, the stabilizer is selected from at least one of lead 2-ethyl acetate, lead salicylate, lead stearate tribasic, and lead phthalate dibasic.
In one embodiment, the colorant is selected from barium sulfate, titanium oxide, or iron sulfate.
In one embodiment, the filler is carbon black.
The preparation method of the moisture-curing polyurethane hot melt adhesive is characterized by comprising the following steps:
weighing the raw materials according to the components of the moisture curing type polyurethane hot melt adhesive;
mixing polyethylene glycol 200, 1, 4-butanediol, ethyltrichlorosilane, cerium trichloride and polyisocyanate, reacting for 4-6 h at the temperature of 30-60 ℃ under the condition of protective gas to obtain Si-O-containing polyurethane with the molecular weight of 10-20 ten thousand, adding the plasticizer, the stabilizer and the antioxidant, mixing, and uniformly dispersing to form a semi-finished product base material;
and adding the catalyst, the filler and the colorant into the semi-finished base material, uniformly dispersing and defoaming to obtain the composite material.
The invention has the following beneficial effects:
the moisture curing type polyurethane hot melt adhesive disclosed by the invention has the advantages that the curing speed of the whole formula system can be improved and the operability is improved by selecting the polyethylene glycol 200, the 1, 4-butanediol, the ethyl trichlorosilane and the polyisocyanate, matching with the plasticizer, the catalyst, the filler and the antioxidant in a specific ratio and matching with the rare earth synergistic catalysis of the cerium trichloride, so that the moisture curing type polyurethane hot melt adhesive obtained integrally is Si-O-containing polyurethane, has the characteristics of strong initial adhesion, high bonding strength and good toughness, has extremely strong permeability and affinity, can resist high temperature and can be suitable for firmly bonding base materials such as metal, plastic, glass and the like. Particularly, the catalyst is screened into the nano titanium dioxide and/or the nano calcium carbonate, has large specific surface area, good surface activity and better catalytic activity, and can be used as a filler to improve the toughness and color of the moisture-cured polyurethane hot melt adhesive, improve the solid content and facilitate the sizing. The preparation method of the moisture curing type polyurethane hot melt adhesive is simple and reliable, and the gluing is convenient.
Furthermore, by screening the specific types and proportions of the plasticizer, the catalyst, the filler, the antioxidant and the colorant, the overall adhesive strength of the moisture-curable polyurethane hot melt adhesive is higher than that of a conventional adhesive under the same condition under the condition of low use amount of the moisture-curable polyurethane hot melt adhesive, and the use amount of the adhesive can be remarkably reduced. The moisture curing type polyurethane hot melt adhesive is convenient to glue, has a low melting point, can be glued at 110 ℃, reacts with moisture in moisture, has very high impact resistance, and can be widely applied to electronic products such as narrow frames of mobile phones and tablet computers.
Detailed Description
The moisture-curable polyurethane hot melt adhesive and the preparation method thereof according to the present invention will be described in further detail with reference to the following specific examples.
Example 1
This example provides a moisture-curable polyurethane hot melt adhesive, which comprises the raw materials in the weight parts in table 1. The preparation method of the moisture-curable polyurethane hot melt adhesive comprises the following steps:
weighing the raw materials according to the components of the moisture curing type polyurethane hot melt adhesive in the table 1.
Polyethylene glycol 200, 1, 4-butanediol, ethyltrichlorosilane, cerium trichloride and polyisocyanate react for 5 hours at 40 ℃ under the condition of protective gas to obtain Si-O-containing polyurethane with the molecular weight range of 10-20 ten thousand, and then a plasticizer, a stabilizer and an antioxidant are added and mixed, and are uniformly dispersed to form a semi-finished product base material. And adding a catalyst, a filler and a coloring agent into the semi-finished base material, uniformly dispersing and defoaming to obtain the composite material.
Table 1 composition of moisture-curable polyurethane hotmelt adhesive of example 1
Example 2
This example provides a moisture-curable polyurethane hot melt adhesive, which comprises the raw materials in the weight parts in table 2. The preparation method of the moisture-curable polyurethane hot melt adhesive of this example was the same as that of example 1.
Table 2 composition of moisture-curable polyurethane hotmelt adhesive of example 2
Example 3
This example provides a moisture-curable polyurethane hot melt adhesive, which comprises the raw materials in the weight parts in table 3. The preparation method of the moisture-curable polyurethane hot melt adhesive of this example was the same as that of example 1.
Table 3 composition of moisture-curable polyurethane hotmelt adhesive of example 3
Example 4
This example provides a moisture-curable polyurethane hot melt adhesive, which comprises the raw materials in the weight parts in table 4. The preparation method of the moisture-curable polyurethane hot melt adhesive of this example was the same as that of example 1.
Table 4 composition of moisture-curable polyurethane hotmelt adhesive of example 4
Example 5
This example provides a moisture-curable polyurethane hot melt adhesive, which comprises the raw materials in the weight parts in table 5. The preparation method of the moisture-curable polyurethane hot melt adhesive of this example was the same as that of example 1.
TABLE 5 composition of moisture-curable polyurethane hotmelt adhesive of example 5
Comparative example 1
The comparative example provides a moisture-curable polyurethane hot melt adhesive comprising the raw materials in parts by weight in table 6. The preparation method of the moisture-curable polyurethane hot melt adhesive of this comparative example was the same as that of example 1.
TABLE 6 composition of moisture-curable polyurethane hotmelt adhesive of comparative example 1
Comparative example 2
The comparative example provides a moisture-curable polyurethane hot melt adhesive comprising the raw materials in parts by weight in table 7. The preparation method of the moisture-curable polyurethane hot melt adhesive of this example was the same as that of example 1.
TABLE 7 composition of moisture-curable polyurethane hotmelt adhesive of comparative example 2
Comparative example 3
The comparative example provides a moisture-curable polyurethane hot melt adhesive comprising the raw materials in parts by weight in table 8. The preparation method of the moisture-curable polyurethane hot melt adhesive of this comparative example was the same as that of example 1.
TABLE 8 composition of moisture-curable polyurethane hot melt adhesive of comparative example 3
Performance testing
The properties of the moisture thermosetting polyurethane hot melt adhesives of examples 1 to 5 and comparative examples 1 to 3 were tested, and the results are shown in Table 9.
TABLE 9 Properties of the moisture-curable polyurethane hotmelts of examples 1 to 5 and comparative examples 1 to 3
As can be seen from Table 9, compared with comparative examples 1 to 3, the moisture-curable polyurethane hot melt adhesives of examples 1 to 5 have good adhesive strength and impact strength and high temperature resistance under the condition that the construction materials are less or the same.
The technical features of the embodiments described above may be arbitrarily combined, and for the sake of brevity, all possible combinations of the technical features in the embodiments described above are not described, but should be considered as being within the scope of the present specification as long as there is no contradiction between the combinations of the technical features.
The above-mentioned embodiments only express several embodiments of the present invention, and the description thereof is more specific and detailed, but not construed as limiting the scope of the invention. It should be noted that, for a person skilled in the art, several variations and modifications can be made without departing from the inventive concept, which falls within the scope of the present invention. Therefore, the protection scope of the present patent shall be subject to the appended claims.
Claims (9)
1. The moisture-curing polyurethane hot melt adhesive is characterized by comprising the following raw materials in parts by weight:
wherein the polyisocyanate is 8 parts of MDI and 20 parts of HDI, the plasticizer is 5 parts of di-n-octyl phthalate and 4 parts of dicyclohexyl phthalate, and the filler is carbon black.
2. The moisture-curable polyurethane hot melt adhesive according to claim 1, wherein the molecular weight of the moisture-curable polyurethane hot melt adhesive is 10-20 ten thousand.
3. The moisture-curable polyurethane hot melt adhesive according to claim 1 or 2, wherein the colorant is selected from titanium oxide.
4. The moisture-curable polyurethane hot melt adhesive according to claim 1 or 2, wherein the antioxidant is at least one selected from the group consisting of 4-hydroxyoctadecanoic acid anilide, 4 '-thiobis (3-methyl-6-tert-butylphenol), and 2, 2' -methylenebis (4-methyl-6-tert-butylphenol).
5. The moisture-curable polyurethane hot melt adhesive according to claim 1 or 2, wherein the stabilizer is at least one selected from the group consisting of lead 2-ethylacetate, lead salicylate, lead stearate tribasic, and lead diphthalate.
6. The moisture-curable polyurethane hot melt adhesive according to claim 1 or 2, wherein the colorant is selected from barium sulfate.
7. The moisture-curable polyurethane hot melt adhesive according to claim 1 or 2, wherein the antioxidant is 4-hydroxyoctadecanoic acid anilide.
8. The moisture-curable polyurethane hot melt adhesive according to claim 1 or 2, wherein the colorant is selected from iron oxides.
9. A method for preparing the moisture-curable polyurethane hot melt adhesive according to any one of claims 1 to 7, which is characterized by comprising the following steps:
weighing the raw materials according to the components of the moisture-curing polyurethane hot melt adhesive as defined in any one of claims 1 to 7;
mixing polyethylene glycol 200, 1, 4-butanediol, ethyltrichlorosilane, cerium trichloride and polyisocyanate, reacting for 4-6 h at the temperature of 30-60 ℃ under the condition of protective gas to obtain Si-O-containing polyurethane with the molecular weight of 10-20 ten thousand, adding the plasticizer, the stabilizer and the antioxidant, mixing, and uniformly dispersing to form a semi-finished product base material;
and adding nano titanium dioxide, nano calcium carbonate, the filler and the colorant into the semi-finished base material, uniformly dispersing and defoaming to obtain the composite material.
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| CN109627414B (en) * | 2018-12-11 | 2021-08-24 | 长春安旨科技有限公司 | High-temperature post-curing polyurethane composite material |
| CN109768123B (en) * | 2019-01-31 | 2022-10-14 | 泰州隆基乐叶光伏科技有限公司 | Welding method |
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